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A catalytic amount of Zeise's dimer and 15‐crown‐5 were combined to effectively promote the regioselective formation of β‐alkoxy ketones from 2‐(homopropargyloxy)ethanols in dimethoxyethane. The desired products were obtained in 59–98 % yields with up to 17:1 exo/endo regioselectivity. The methodology allows access to β‐hydroxy ketones as an aldol reaction alternative.
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